CN103547348A - Process for production of sulphuric acid - Google Patents
Process for production of sulphuric acid Download PDFInfo
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- CN103547348A CN103547348A CN201280016203.9A CN201280016203A CN103547348A CN 103547348 A CN103547348 A CN 103547348A CN 201280016203 A CN201280016203 A CN 201280016203A CN 103547348 A CN103547348 A CN 103547348A
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- process gas
- condenser
- heat transfer
- transfer medium
- condensation
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- 238000000034 method Methods 0.000 title claims abstract description 173
- 230000008569 process Effects 0.000 title claims abstract description 149
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 235000011149 sulphuric acid Nutrition 0.000 title claims abstract description 16
- 239000001117 sulphuric acid Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 64
- 230000005494 condensation Effects 0.000 claims abstract description 63
- 238000012546 transfer Methods 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims description 33
- 238000007669 thermal treatment Methods 0.000 claims description 28
- 238000013459 approach Methods 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000007800 oxidant agent Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 122
- 230000008901 benefit Effects 0.000 description 32
- 239000007788 liquid Substances 0.000 description 18
- 238000004581 coalescence Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 17
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000011144 upstream manufacturing Methods 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 229920002313 fluoropolymer Polymers 0.000 description 3
- 239000004811 fluoropolymer Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- -1 sulphur compound Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
- F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0036—Flash degasification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0039—Recuperation of heat, e.g. use of heat pump(s), compression
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/765—Multi-stage SO3-conversion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/80—Apparatus
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/76—Preparation by contact processes
- C01B17/80—Apparatus
- C01B17/806—Absorbers; Heat exchangers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L53/00—Heating of pipes or pipe systems; Cooling of pipes or pipe systems
- F16L53/30—Heating of pipes or pipe systems
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L55/00—Devices or appurtenances for use in, or in connection with, pipes or pipe systems
- F16L55/02—Energy absorbers; Noise absorbers
- F16L55/027—Throttle passages
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B39/00—Evaporators; Condensers
- F25B39/04—Condensers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/2931—Diverse fluid containing pressure systems
- Y10T137/3003—Fluid separating traps or vents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention relates to a condenser, having a process gas side and a heat transfer medium side said condenser being configured for feeding a hot process gas containing a condensable component to an inlet of the condensing side, and being further configured for withdrawing a cooled process gas from an outlet of the condensing side, and being even further configured for withdrawing a condensate in a position proximate to one end of the condenser, and said condenser having the process gas side divided in a process gas cooling zone configured for having a cool heat transfer medium inlet and a heated heat transfer medium outlet, and a process gas re-heating zone downstream the process gas cooling section, configured for re-heating of the process gas, as well as a processes for condensation and production of sulphuric acid employing such a condenser.
Description
The present invention relates to a kind ofly be designed for the condenser of avoiding condensed downstream problem, and adopt described condenser for adopting condensation of sulfuric acid device by thering is 0.1-30% SO
2and SO
3(SO
x) the feed gas process of producing the concentrated sulfuric acid and oleum.Feed gas can be derived from sulphur and sulphur compound burning, from wet washing, be derived from the SO of metal sulfide baking
2the heat regeneration of gas, the sulfuric acid of using by oneself and sulfate or from being rich in H
2the gas that the burning of the flue gas of S produces.In feed gas up to 99.995% SO
xrecyclable for to be generally the concentrated sulfuric acid of 95-99.5 % by weight and/or to have up to 25 % by weight SO
3oleum.By guaranteeing the condition that is unfavorable for sulfuric acid droplets condensation in condenser outside, method of the present disclosure relates to avoids the corrosion of hot sulfuric acid droplets in process device.
Known to two-step catalysis SO
2transform and intermediate absorption SO in the middle of relating to and in the process of final absorption or condensing steps
3or condensation H
2sO
4, by containing up to 30 volume % SO
2strong SO
2the gas generation concentrated sulfuric acid, wherein SO
2conversion ratio is up to 99.9% or more.In principle, by absorb SO in liquid phase
3, by the SO in gas phase
3be transferred to liquid phase, and by condensation, by H
2sO
4vapor transfer is to liquid phase, wherein by directly contacting with as the recycle acid of cooling agent or in falling liquid film condenser, by gas cooled to lower than its sulphuric acid dew point, in described condenser by gas cooled to lower than its dew point, and acid condensation on the surface of air cooled glass tube.
Our U.S. Patent number 7,361,326 discloses for by having up to 30% SO
2and H
2o/SO
2ratio is greater than two condensation processes that approximately 1 feed gas is produced the concentrated sulfuric acid.In the first step of this process, most of SO
2be converted into SO
3, subsequently process gas is led to interconderser, wherein in by the cooling packed column of recycle acid or in vertical air cooled glass tube, SO
3and H
2sO
4steam condensing is the concentrated sulfuric acid, and wherein process gas upwards flows or flows downward in described pipe.The latter is as avoiding the option of liquid flooding to be mentioned under high gas velocity, but be considered to bring its production to there is the shortcoming of the sulfuric acid of low concentration (70-85 % by weight), therefore need enriching stage subsequently, packed column for example, to reach the sulfuric acid concentration of 95 % by weight or above expectation.Make the process gas leaving from interconderser through the 2nd SO
2step of converting, and adding under particle subsequently, lead to final wet condensation stage.
In the prior art, according to the character of condenser, the process gas stream that flows out condenser glass tube in or approach the gas of condensing condition.The dense H of condensation
2sO
4high corrosion.Therefore, for this part of procedure layout, at least for example by before overcoming condensing condition with Dilution air or heating process stream, must be with liner surface or the expensive equipment of being made by glass.
Similarly, can be relevant to the less desirable condensation in condenser downstream and then from the output of condenser in other arranges, there is negative chemistry or corrosive effect.
Therefore, an object of the present disclosure is to overcome the shortcoming relevant to prior art, and wherein essential design intermediate equipment, to overcome the negative results of condensation, for example, needs to bear condensation sulfuric acid condition.
By providing the condenser that comprises following part to meet this object: the temperature that wherein process gas that contains condensable components is heated to again surpass condensing condition, make from the condenser mobile not condensation of process gas of equipment downstream, and the in the situation that of the condensable liquid of corrosivity, equipment can be prepared by standard carbon steel.
With regard to the application's object, should adopt following term:
The dew point of gas component is the temperature/pressure of component during from admixture of gas condensation.
The gas that contains one or more condensable components under condition Y under condition X is interpreted as following composition: lower at condition X (temperature and pressure) is gaseous state, but under condition Y (lower temperature and/or higher pressure), a part is using condensation as liquid.When not mentioned condition (gas that contains one or more condensable components), condition Y is assumed to atmospheric pressure and room temperature, and condition X is assumed to higher temperature and/or lower pressure, makes gas " surpass dew point ", i.e. not condensation.Term " condensable gases " is interpreted as the gas that contains one or more condensable components under room temperature and atmospheric pressure.
" condenser " is interpreted as wherein between warm process gas and heat transfer medium, occurring the process unit of heat exchange, if make this warm process gas contain condensable components, this component is at condenser internal condensation.
The condenser side of the process gas stream that " condensation side of condenser or Process Gas side " is interpreted as being provided for containing condensable components stream, no matter whether condition makes in fact to occur condensation.
" the heat transfer medium side of condenser " is interpreted as the wherein condenser side of heat transfer medium flows.
" condensate " is interpreted as the liquid forming by the cooling gas that contains condensable components.
" with respect to the upstream of a certain position " is interpreted as in typical operating period in more approaching the position of entrance.
" with respect to the downstream of a certain position " is interpreted as in the position of typical operating period in more approaching outlet.
For condenser unit, upstream portion and downstream part should limit by the typical flow direction of Process Gas side rather than heat transfer medium." upstream process gas cooled district " is interpreted as the district on the Process Gas side of condenser, and it approaches the entrance that process gas leads to condenser." downstream process gas cooled district " is interpreted as the district on the Process Gas side of condenser, and it approaches the outlet that process gas leaves condenser.
" process gas is the thermal treatment zone again " is interpreted as wherein the district on the Process Gas side of the condenser of heating process gas again.
Counter-current flow is interpreted as wherein said being flowing on the contrary or two streams in contrary direction substantially.
Cross-flow is interpreted as wherein said two streams that are flowing in vertically or in the direction of perpendicular.
In whole application, compound can be referred to by chemical formula, chemical name or popular name.These are interpreted as complete synonym, and should not give special implication by the difference on this term.
According to the present invention, by thering is the condenser of Process Gas side and heat transfer medium side, meet the object of avoiding condensation problem,
Described condenser is set to the hot process gas that contains condensable components to the entrance charging of condensation side,
And be further set to take out cooling process gas from the outlet of condensation side,
And be even further set to take out condensate in the position that approaches one end of condenser,
And described in there is Process Gas side condenser be divided into process gas cooling zone and the process gas thermal treatment zone again, described process gas cooling zone arranges has cold heat transfer medium inlet and through heating heat transfer medium outlet,
The thermal treatment zone is in process gas cooling segment downstream again for described process gas, and it is set to heating process gas again, and associated benefits is to leave the process gas not condensation substantially of condenser.
Being arranged so that process gas, the Process Gas side of the thermal treatment zone is from accepting another embodiment of heat energy through heating heat transfer medium again, and associated benefits is the thermal efficiency being improved by being recovered in the heat that discharges in condenser.
Another embodiment is set to heat transfer medium and the process gas counter-current flow in the thermal treatment zone again, and relevant benefit is the improved heat transfer from heat transfer medium to process gas.
In another embodiment, condenser is set to heat transfer medium in the thermal treatment zone and process gas with cross-flow operation again, and relevant benefit is again the simple physical arrangement of the thermal treatment zone.
In another embodiment, condenser is set to approach process gas entrance and takes out condensate, and relevant benefit is improved condensation efficiency, thereby avoids subsequently concentrated of condensate.
In another embodiment, condensate comprises sulfuric acid or oleum, and the above-mentioned benefit for sulfuric acid or oleum production process is provided specifically.
In another embodiment, condenser is set to Process Gas side to be separated by glass and heat exchange medium, and relevant benefit is the corrosion resistance of high level in condenser.
In another embodiment, condenser comprises glass tube, it is set to have process gas stream on the inner side of glass tube and on the outside of glass tube, has heat transfer medium stream, and relevant benefit is the high surface at the hot interface between Process Gas side and heat transfer medium side.
In another embodiment, condenser comprises glass tube, and it is set to have heat transfer medium stream on the inner side of glass tube and has process gas stream on the outside of glass tube, and relevant benefit is that the physical orientation of glass tube and the taking-up of condensate are irrelevant, for example, allow horizontal mounting glass pipe.
In another embodiment, condenser also comprise by condensing zone and again the heat transfer medium flow point in the heat transfer medium side of the thermal treatment zone every flow restriction element, relevant benefit be condensing zone and again the heat of the thermal treatment zone separate.
In another embodiment, flow restriction element comprises one or more stable elements that are connected with metallic plate, relevant benefit is the high-voltage stability that obtains flow restriction element, and compares with the bulk board with uniform pressure stability, only needs limited amount material.
In another embodiment, condenser also comprises one or more turbulent flows and strengthens element, and relevant benefit is to provide process gas and contacts with the improved of tube wall.
In another embodiment, condenser also comprises one or more retaining elements, independent recess for example, and relevant benefit is to provide the means that position element are fixed on to the inside of pipe and pipe had to minimum change.
In another embodiment, condenser also comprises fixing shoulder, and it is a part with the glass tube of less internal cross-sectional area, and relevant benefit is to provide the means that position element are fixed on to the inside of pipe and do not jeopardize the overall exterior shape of pipe.
In another embodiment, one or more turbulent flows strengthen element and are set to by hanging and fix from retaining element, and relevant benefit is to avoid the weight that strengthens element due to turbulent flow to make droplet coalescence deformed element.
In another embodiment, one or more turbulent flows strengthen element and are set to fix by being placed on retaining element, and relevant benefit is to avoid turbulent flow to strengthen the tensile stress in element.
In another embodiment, condenser also comprises droplet coalescence element, and relevant benefit is mist and droplet coalescence, makes condensation maximizing before heating process gas again.
In another embodiment, retaining element engages droplet coalescence element, makes the movement of restricting liquid drop coalescing element, and relevant benefit is that droplet coalescence element is fixed on the heating process gas position of condensation maximizing before again.
In another embodiment, condenser also comprises limiting element, and it is set to the movement of restricting liquid drop coalescing element, and relevant benefit is the further fixing position of drop coalescing element.
At condenser, have in pipe shoulder another embodiment as retaining element, limiting element also comprises one or more film-shaped devices narrow and wide end that have, and described film-shaped device is set to for making the fixedly shoulder mechanical engagement of its wide end and tube wall, make the mobile restricted system of limiting element, relevant benefit is the fixing position of drop coalescing element, on the droplet coalescence element of combination and retaining element, has minimum extra pressure loss.
At condenser, have in one or more pipe recesses another embodiment as retaining element, limiting element also comprises ring-type element, described ring-type element is set to for making its periphery and retaining element mechanical engagement, make the mobile restricted system of limiting element, relevant benefit is to contact with whole tube wall periphery is stable.
An alternative enforcement of the present invention is a kind of method of sulfuric acid and/or oleum for condensation process gas, said method comprising the steps of:
(i) process gas is led to according to the condensation of sulfuric acid of the present disclosure stage, wherein inlet temperature surpasses the dew point of sulfuric acid,
(ii) process gas is cooled to the dew point lower than sulfuric acid,
(iii) condensation and taking-up sulfuric acid, and
(iv) at condenser, in the stage, heating process gas is to surpassing sulphuric acid dew point again, and compared with prior art, its associated benefits is, because the risk of condensed downstream is removed, so reduce the requirement to condenser downstream resistant material.
In another embodiment, after heating again in step (iv), temperature at the exit in condenser stage process gas surpasses at least 10 ℃ of sulphuric acid dew points, relevant benefit is, because the risk of condensed downstream is removed, there is enough margin of safetys, so reduce the requirement to condenser downstream resistant material.
Another alternative enforcement of the present invention relates to a kind of method for the production of the sulfuric acid in process gas and/or oleum, said method comprising the steps of:
(a) provide the SO that contains 0.1-30 % by mole
2fill process gas;
(b) make fill process gas through a SO
2step of converting, wherein in one or more catalyst beds, SO
2be oxidized to SO
3;
(c) will be from a described SO
2step of converting contain SO
3process gas be cooled to the temperature of sulphuric acid dew point 0-100 ℃ over process gas; With
(d) sulfuric acid in condensation process gas in the first condensation phase,
The wherein said condenser stage operates according to the disclosure, and relevant benefit is to provide benefit of the present disclosure for producing sulfuric acid.
In another embodiment of the present invention, further comprising the steps of for the production of the method for the sulfuric acid in process gas and/or oleum:
(e) further heat again the resulting process gas stream from step (f), and make this process gas lead to the 2nd SO
2step of converting, wherein in one or more catalyst beds, remaining SO
2be oxidized to SO
3,
(g) process gas is cooled to the temperature over 0-100 ℃ of its sulphuric acid dew point, and
(h) subsequently process gas is led to final condensation phase,
Wherein the condenser stage (d) and (h) at least one according to the disclosure, operate, relevant benefit is to provide the sulfur dioxide of improving the standard and removes.
The inlet temperature that another embodiment relates to the process gas that leads to the second catalyst unit is 350-470 ℃, preferably 350-400 ℃, or preferred 350-370 ℃, relevant benefit is the requirement of coupling catalyst bed, guarantee thermal balance and the minimum amount temperature of crossing optimized, this guarantees SO simultaneously
2/ SO
3balance optimization.
The inlet temperature that another embodiment relates to the process gas that leads to the second catalyst unit is 400-470 ℃, preferred 400-450 ℃, and relevant benefit is to provide high reaction rate, thereby allows little catalyst bed.
Another embodiment relates to and adds rich O
2the oxidant of the form of gas, for example pure O
2, benefit is, compares with atmospheric air, adds less inert gas, this causes the reduction size of process device again, thereby causes the cost that reduces.
With reference to accompanying drawing, by the following description of the embodiment preferred form providing as limiting examples, these and other characteristic of the present disclosure will be clear, wherein:
Fig. 1 shows according to prior art by containing SO
2process gas produce H
2sO
4procedure layout,
Fig. 2 shows according to an embodiment of the present disclosure, adopts condenser of the present disclosure, by containing SO
2process gas produce H
2sO
4procedure layout,
Fig. 3 shows the condenser tube for embodiments more of the present disclosure,
Fig. 4 demonstration comprises the pipe for the retaining element of embodiments more of the present disclosure, and
Fig. 5 shows the example for the limiting element of embodiments more of the present disclosure.
Adopt 2 condensing steps, for SO
2the process according to prior art of oxidation and the condensation concentrated sulfuric acid is subsequently shown in figure l.The key step of this process is included in the SO in the first catalytic reactor 140 under the first catalyst existence
2oxidation, the SO that condensation produces in interconderser 142
3as sulfuric acid, in the second catalytic reactor 144, be oxidized remaining SO
2, and in final condenser 146 further condensation of residual with the SO producing
3, substantially clean process gas can be delivered to atmosphere subsequently.
In this process, it is essential that temperature is controlled, especially because of SO in 140 and 142
2to SO
3heat release catalytic oxidation need minimum temperature, and high temperature limit SO
2with SO
3between balance, make a part of SO
2by can not be oxidized at higher temperature.Easily by H
2o and SO
3the how liquid H forming
2sO
4have very much corrosivity, and quite different at gaseous state, therefore expectation keeps containing H
2sO
4process gas surpass dew point until condensation is condensate in and needs in essence temperature lower than dew point, therefore need resistant material, for example glass tube.Particularly, the inlet temperature of this Process Design catalyst bed is 370-500 ℃, and the inlet temperature of condenser 142 is 5-100 ℃, and preferred 10-70 ℃, or even more preferably 20-50 ℃, for example, surpass approximately 30 ℃ of sulphuric acid dew points.
In a specific embodiments of this process, guide process gas 100 into first catalytic reactor 140, wherein there are most of SO
2oxidation.This first catalytic reactor can design has a catalytic bed or a plurality of catalytic bed, if the amount of sulfur dioxide is very high, expectation is for example taken out reaction heat in heat exchanger 130 and 132, to provide reaction at the temperature reducing, make the entry process gas 102 that leads to the first condenser 142 not be subject to SO
2with SO
3between the restriction of balance.
In interconderser 142, if SO
3be condensed into H
2sO
4, at outlet 106 places, SO
3concentration enough height make to corrode.
It is the process gas 102 of 290 ℃ that interconderser 142 is set to the cooling representative temperature that enters condenser.Conventionally by for example, carrying out coolingly with heat transfer medium (air 120) heat exchange, this heat transfer medium is in the temperature lower than process gas.Condenser 142 is must setting compatible with condensate with process gas, and for corrosivity condensable components, this can comprise corrosion-resistant, for example, for example, by glass tube or other resistant material (earthenware or use protective coating lining), is made.
Conventionally cooling zone 150 is heat exchanger, and wherein heat transfer medium (for example air) adverse current flows to process gas.The benefit of counter-current flow is, at the flow direction of process gas, temperature will reduce, so the potentiality of condensation will improve.Thereby obtain the condensation of highest level.
Conventionally condenser is provided with process gas entrance 102 in bottom vertical, and in bottom, collects the liquid 114 of condensation, but in the situation that process gas stream is very high, can preferably make the liquid stream and gas stream of condensation, to avoid overflow.
According to prior art, operation condenser, makes all positions at condenser, condition in or approach the dew point of condensable components.This is the natural result of counter-current operation, because the temperature of (except after entrance immediately) is all in condensing condition in all positions of condenser, and in downstream more, temperature is always lower.
Now, as illustrated in fig. 2, developed the alternative of prior art, comprised according to condenser 142 of the present disclosure, the process gas that wherein connects heating process gas wherein behind process gas cooling zone 150 is the thermal treatment zone 152 again.In order to ensure successfully heating, the heat transfer medium of cooling zone must be separated with the thermal treatment zone more again.A kind of mode of doing is like this that blocking-up heat transfer medium flows to the thermal treatment zone again from cooling zone.Secondly, be necessary for the thermal treatment zone thermal source is provided.For the thermal treatment zone 152 provides a kind of possible mode of heat, being will from the upstream portion of condenser, to be transferred in the process gas of the downstream of the condenser heat transfer medium side of the thermal treatment zone 152 again through heating heat transfer medium in pipeline 122, is for example cross-flow, and the mobile process gas that arranges on heating process gas side of stream or counter-current flow thereby take with respect to process gas.
In specific embodiments of the present disclosure, for H
2sO
4/ SO
3the process of condensation, Process Gas side and heat transfer medium side can be flowed and separate by a side in glass tube, so that corrosion resistance to be provided.
In one embodiment, heat transfer medium stream can be inner at glass tube, and sulfuric acid is in the external condensation of pipe.In this arranges, heat transfer medium stream limits by the connection of pipe, and therefore, it is simple which part of control condenser is fetched through heating heat transfer medium.In this arranges, heating tube preferred levels is arranged, by producing maximum turbulent flow, is made them have the heat exchanger effectiveness of optimization.In this arranges, condenser wall must be made by height resistant material.
In an alternate embodiment, at the stream of glass tube inside for containing condensable H
2sO
4process gas, make to occur in the inside of pipe condensation, and can collect condensate in the bottom zone of condenser, it can be positioned at gas access horizontal plane or lower than gas access, approach the end of condenser.In this case, the flow restriction element 154 in heat transfer medium side is useful, to guarantee avoiding entering the process gas heat transfer medium side of the thermal treatment zone 152 again for the cold heat transfer medium of cooling procedure gas in cooling segment 150.Must recognize, when will be through heating heat transfer medium while guiding again thermal treatment zone gas into, pressure on the cold side of flow restriction element 154 conventionally can be higher than the pressure in warm side, therefore flow restriction element 154 must be designed to substantially flow and seal for heat transfer medium, for example, for example, by the resistant material packing ring of (fluoropolymer, comprises PTFE or PFA) is provided, but do not need positive confinement.
Or, except other thermal source heat transfer medium can be used as the thermal source of the thermal treatment zone 152 again through heating, be mainly other warm process gas, still can use any other heater means, for example electrical heating.
For wherein process gas is at the condenser of glass tube internal flow, flow restriction element 154 conducts that can prepare in heat transferring medium side divide tube sheets, wherein arrange and manage the hole of mating.Particularly, divide tube sheet to make or to be made by the flake structure based on steel plate with stabilizer by steel plate.When condensable components has corrosivity, plate can be made by corrosion resisting steel or another kind of resistant material, or it can for example, carry out surface protection by suitable material (fluoropolymer, comprises PTFE or PFA).
In the prior art, for SO
3the detailed process of condensation, condenser is made out of tubes conventionally, and described pipe for example, is made by resistant material (glass).It is round that pipe is generally.In the inside of pipe, turbulent flow is installed conventionally and strengthens element (for example spiral) to contribute to heat transfer and condensation, and provide material plug to help the condensation of condensable liquid.
According to the disclosure, for H
2sO
4/ SO
3the detailed process of condensation, condenser Process Gas side is made by resistant material (being generally glass tube), but also can use pipe or other geometry of being made by the material of pottery or coating.Pipe can be round conventionally, but they can have any suitable shape.As illustrated in fig. 3, manage 300 and can be set to be provided with turbulent flow enhancing element (for example spiral 306), by forming turbulent flow, help to conduct heat, there is the minimum pressure loss.In addition, pipe also can be set to provide droplet coalescence element 302, demister for example, i.e. and material plug, to help drop to form, thus the condensable liquid of condensation.By introduce the thermal treatment zone in condenser, pipe is preferably set to be furnished with droplet coalescence element in the downstream that approaches cooling segment, and pipe also can be set to be furnished with the second turbulent flow enhancing element 304,308 in heating part.
When use disclosed condenser in condensation process, wherein process gas is when glass tube 300 internal flow, and it can be set to comprise process supporting element valuably, for example, in the inner turbulent flow of pipe, strengthen element, for example spiral 304,306,308, and droplet coalescence element 302.These process supporting elements are not that operation of the present disclosure is necessary, but their existence can have contribution to efficiency of the present disclosure.In addition, the concrete setting of condenser can comprise for keeping these process supporting elements at the element of tram.
Such condensation process strengthens element and also can use with the benefit in other condensation process.
For example, the condensable liquid of condensate corrosion (sulfuric acid) in the situation that, process supporting element can for example, be made by height resistant material (fluoropolymer, comprises PTFE or PFA) valuably.
Approach the outlet of the condensing zone of condenser tube, can arrange droplet coalescence element 302.Although on the one hand, importantly the pressure loss on droplet coalescence element is low, but also importantly, before the thermal treatment zone, droplet coalescence element can be collected the mist of condensable components and the signal portion of drop, to guarantee that the liquid of condensation is not reheated and evaporates, but be collected as the drop of condensate.
By the retaining element in pipe, can guarantee that turbulent flow strengthens the location of element.These retaining elements can comprise one or more partially or completely restrictions to glass tube internal diameter, comprise the independent recess 406 of glass tube, as shown in Figure 4, or the shoulder 410 forming by reducing the diameter of glass tube.Retaining element can strengthen upstream or the downstream layout of element 304,306,312 in turbulent flow, make to be placed on retaining element or by hanging from retaining element by turbulent flow being strengthened to element, and fixedly turbulent flow strengthens the position of element.
Also may be useful, the movement of coalescent 302 elements of restricting liquid drop, makes condensation process gas not change the position of droplet coalescence element.As at Fig. 3 and illustrated in fig. 4, can realize this point by managing one or more recesses of 306,310,406,410, comprise and form shoulder 310,410.In addition, condenser can be set to droplet coalescence element 302 and place on other limiting element 306, one or more recesses of limiting element 306 contact pipes, and support droplet coalescence element, or as illustrated in Fig. 3 A, wherein turbulent flow strengthens the fixedly position of drop coalescing element 302 of element 304.In Fig. 5, the instantiation that shows the limiting element that these are other, comprise and be set to be placed on the ring on one or more recesses, for example 500 and 502, or in the situation that the shoulder of pipe shrinks, limiting element and tube wall only have contact point seldom, for example, be set to be placed on plate 504, the cross-member 506 that pipe shrinks, the element 510 that has outstanding ring 508 or extend, and around them, can arrange droplet coalescence element.For all these elements, common is moving freely of their restricting liquid drop coalescing elements, the position of droplet coalescence element is suitably limited, and completed condensation before drop enters the thermal treatment zone again.
Use another benefit of disclosed condenser to comprise as flue (stack) final condenser before.In the prior art, common practice is to add hot diluent air in this position, to avoid H
2sO
4condensation, but according to the heat energy recycling in condenser of the present disclosure in heat transfer medium, more effectively avoiding these problems.
Embodiment
embodiment 1
According to the first exemplary of prior art, be included in WSA sulphuric acid device and process and contain H
2the tail gas of S.This process is comprised of 3 steps:
A) burning, H
2s is oxidized to SO
2
B) SO
2transform SO
2with O
2reaction and be converted into SO
3
C) condensation, SO
3hydration is H
2sO
4(gas), and be condensed into H
2sO
4(liquid)
According to Fig. 1, this process operates under the process condition shown in table 1, makes the process gas outlet temperature of condenser lower than sulphuric acid dew point, and condenser downstream needs resistant material.
Table 1
Process gas leaves condenser at 110 ℃, lower than approximately 18 ℃ of sulphuric acid dew points.Therefore, the liquid drop that it contains sulfuric acid, makes it have very much corrosivity.
embodiment 2
According to the second exemplary of the present disclosure, be shown in Fig. 2 and table 2.Condition is corresponding to those of embodiment 1 herein, and just condenser operates according to the disclosure, for example, has the thermal treatment zone again, makes the process gas outlet temperature of condenser surpass sulphuric acid dew point, makes condenser downstream needn't use resistant material.
Table 2
In this embodiment, process gas leaves condenser at 180 ℃, and it surpasses approximately 50 ℃ of sulphuric acid dew points.Therefore, gas is for dry and no longer have corrosivity.
Claims (15)
1. a condenser with Process Gas side and heat transfer medium side,
Described condenser is set to the hot process gas that contains condensable components to the entrance charging of condensation side,
And be further set to take out cooling process gas from the outlet of described condensation side,
And be even further set to take out condensate in the position that approaches one end of described condenser,
And described in there is Process Gas side condenser be divided into process gas cooling zone and the process gas thermal treatment zone again,
Described process gas cooling zone arranges has cold heat transfer medium inlet and through heating heat transfer medium outlet,
The described process gas again thermal treatment zone, in described process gas cooling segment downstream, is set to heat described process gas again.
2. the condenser of claim 1, wherein said condenser is set to described process gas and from described, through heating heat transfer medium, accepts heat energy in the Process Gas side of the thermal treatment zone again.
3. the condenser of claim 2, its be set to described in again the heat transfer medium in the thermal treatment zone and process gas with counter-current flow.
4. the condenser of claim 2, its be set to described in again the heat transfer medium in the thermal treatment zone and process gas with cross-flow operation.
5. the condenser of any one in the claims, wherein said condensate comprises sulfuric acid or oleum.
6. the condenser of any one in the claims, wherein said condenser is set to described Process Gas side and described heat exchange medium side is separated by glass.
7. the condenser of the claims 6, described condenser comprises one or more glass tubes, and it is set to have process gas stream on the inner side of described glass tube and on the outside of described glass tube, has heat transfer medium stream.
8. the condenser of the claims 7, described condenser comprises one or more glass tubes, and it is set to have heat transfer medium stream on the inner side of described glass tube and has process gas stream on the outside of described glass tube.
9. the condenser of any one in the claims, described condenser also comprises flow restriction element, its by the heat transfer medium flow point in the heat transfer medium side of described condensing zone and the described thermal treatment zone again every.
10. the flow restriction element of the condenser of claim 9, it is provided as the stable element being connected with metallic plate.
11. 1 kinds of methods for sulfuric acid and/or the oleum of condensation process gas, said method comprising the steps of:
(i) described process gas is led to according to the condensation of sulfuric acid stage of any one in claim 1-10, wherein said inlet temperature surpasses the dew point of sulfuric acid,
(ii) described process gas is cooled to the dew point lower than sulfuric acid,
(iii) condensation and taking-up sulfuric acid, and
(iv) at described condenser, in the stage, heat again described process gas to surpassing sulphuric acid dew point.
The method of 12. claims 11, wherein in step (iv) again after heating, surpasses at least 10 ℃ of the dew points of sulfuric acid in the temperature of process gas described in the exit in described condenser stage.
13. 1 kinds of methods for the production of the sulfuric acid in process gas and/or oleum, said method comprising the steps of:
(a) provide the SO that contains 0.1-30 % by mole
2fill process gas;
(b) make described fill process gas through a SO
2step of converting, wherein in one or more catalyst beds, SO
2be oxidized to SO
3;
(c) will be from a described SO
2step of converting contain SO
3process gas be cooled to the temperature of sulphuric acid dew point 0-100 ℃ that surpasses described process gas; With
(d) sulfuric acid in process gas described in condensation in the first condensation phase,
The wherein said condenser stage is according to any one operation in claim 11 or 12.
The method for the production of the sulfuric acid in process gas and/or oleum of 14. claims 13, described method is further comprising the steps of:
(e) further heat again the resulting process gas stream from step (f), and this process gas is led to the 2nd SO
2step of converting, wherein in one or more catalyst beds, remaining SO
2be oxidized to SO
3,
(g) described process gas is cooled to the temperature over 0-100 ℃ of its sulphuric acid dew point, and
(h) subsequently described process gas is led to final condensation phase,
Wherein the condenser stage (d) and (h) at least one according to any one operation in claim 22 or 23.
15. claims 13 or 14 method, wherein said oxidant is with rich O
2the form of gas adds, for example pure O
2.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DKPA201100260 | 2011-04-06 | ||
| DKPA201100260 | 2011-04-06 | ||
| PCT/EP2012/001183 WO2012136307A1 (en) | 2011-04-06 | 2012-03-16 | Process for production of sulphuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103547348A true CN103547348A (en) | 2014-01-29 |
| CN103547348B CN103547348B (en) | 2015-07-22 |
Family
ID=45928802
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|---|---|---|---|
| CN201280016203.9A Expired - Fee Related CN103547348B (en) | 2011-04-06 | 2012-03-16 | Process for production of sulphuric acid |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US8926936B2 (en) |
| EP (1) | EP2694177B1 (en) |
| JP (1) | JP5914631B2 (en) |
| KR (1) | KR101626094B1 (en) |
| CN (1) | CN103547348B (en) |
| AU (1) | AU2012239081B2 (en) |
| CA (1) | CA2830066C (en) |
| CL (1) | CL2013002851A1 (en) |
| EA (1) | EA025201B1 (en) |
| MX (1) | MX2013011484A (en) |
| PE (1) | PE20140486A1 (en) |
| WO (1) | WO2012136307A1 (en) |
| ZA (1) | ZA201306472B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967150A (en) * | 2016-07-08 | 2016-09-28 | 华能国际电力股份有限公司 | Equipment and method for preparing SO3 gas through platinum catalyst |
| CN107848800A (en) * | 2015-07-27 | 2018-03-27 | 奥图泰(芬兰)公司 | Contain SO for cooling down2And/or SO3With the method and apparatus of the gas of water |
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| WO2013182502A1 (en) * | 2012-06-06 | 2013-12-12 | Haldor Topsøe A/S | Process for the oxidation of so2 to so3 |
| JP6310319B2 (en) * | 2014-05-12 | 2018-04-11 | パンパシフィック・カッパー株式会社 | Sulfuric acid factory operating method and sulfuric acid factory operating equipment |
| AU2016287352B2 (en) | 2015-07-02 | 2021-01-07 | Haldor Topsøe A/S | Process for production of sulfuric acid |
| KR102298888B1 (en) * | 2017-03-27 | 2021-09-08 | 현대자동차주식회사 | Humidifier for Fuel Cell |
| AR112622A1 (en) * | 2017-08-08 | 2019-11-20 | Haldor Topsoe As | A PROCESS FOR THE REMOVAL OF AEROSOL DROPS AND A PROCESS PLANT FOR THE PRODUCTION OF SULFURIC ACID |
| KR102298458B1 (en) * | 2017-11-28 | 2021-09-07 | 할도르 토프쉐 에이/에스 | Process for the production of sulfur and sulfuric acid |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2012136307A1 (en) | 2012-10-11 |
| JP5914631B2 (en) | 2016-05-11 |
| EP2694177B1 (en) | 2016-10-05 |
| AU2012239081B2 (en) | 2015-02-19 |
| PE20140486A1 (en) | 2014-05-15 |
| ZA201306472B (en) | 2014-10-29 |
| US20140048228A1 (en) | 2014-02-20 |
| MX2013011484A (en) | 2013-11-04 |
| AU2012239081A1 (en) | 2013-10-17 |
| CN103547348B (en) | 2015-07-22 |
| NZ616169A (en) | 2015-06-26 |
| JP2014512264A (en) | 2014-05-22 |
| KR20140029425A (en) | 2014-03-10 |
| EA201391466A1 (en) | 2014-03-31 |
| CL2013002851A1 (en) | 2014-05-09 |
| CA2830066C (en) | 2015-07-14 |
| KR101626094B1 (en) | 2016-05-31 |
| CA2830066A1 (en) | 2012-10-11 |
| US8926936B2 (en) | 2015-01-06 |
| EA025201B1 (en) | 2016-11-30 |
| EP2694177A1 (en) | 2014-02-12 |
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